CN105815327A - Nanometer titanium dioxide silver-doped composite abamectin pesticide and preparation method - Google Patents
Nanometer titanium dioxide silver-doped composite abamectin pesticide and preparation method Download PDFInfo
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- CN105815327A CN105815327A CN201610265941.7A CN201610265941A CN105815327A CN 105815327 A CN105815327 A CN 105815327A CN 201610265941 A CN201610265941 A CN 201610265941A CN 105815327 A CN105815327 A CN 105815327A
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- titanium oxide
- silver
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- titanium dioxide
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/32—Ingredients for reducing the noxious effect of the active substances to organisms other than pests, e.g. toxicity reducing compositions, self-destructing compositions
Abstract
The invention discloses a nanometer titanium dioxide silver-doped composite abamectin pesticide and a preparation method, belonging to the technical field of composite pesticides. According to the main points of the technical scheme, the method comprises the following steps: adding a nanometer titanium dioxide silver-doped turbid liquid to a stearic acid ethanol solution; carrying out decompression suction filtration on the mixed solution to obtain stearic acid-modified nanometer titanium dioxide silver-doped powder; and adding the stearic acid-modified nanometer titanium dioxide silver-doped powder and cyclohexanone, adding a deionized water solution of lauryl sodium sulfate to avermectin missible oil, and stirring and mixing the solutions to obtain the nanometer titanium dioxide silver-doped composite abamectin pesticide. The technique is simple; industrial production is easy to achieve; the prepared nanometer titanium dioxide silver-doped composite abamectin pesticide has the advantages of being environmentally friendly, short in chemical residue time and the like.
Description
Technical field
The invention belongs to composite pesticide technical field, be specifically related to a kind of nano titanium oxide and mix compound avilamycin pesticide of silver and preparation method thereof.
Background technology
At present, for solving Pesticide Residue, the degraded to avilamycin pesticide does not has good solution, although utilizing nano material to avilamycin of degrading, but its degradation efficiency is low.Therefore, there is a kind of pesticide that can improve degraded avilamycin efficiency to be developed, the effect of parasite killing can either be played, the residence time in crop can be shortened again.
Summary of the invention
Present invention solves the technical problem that there is provided a kind of nano titanium oxide mixes compound avilamycin pesticide of silver and preparation method thereof.
The present invention solves that above-mentioned technical problem adopts the following technical scheme that, a kind of nano titanium oxide mixes the preparation method of the compound avilamycin pesticide of silver, it is characterised in that concretely comprise the following steps:
Step (1), preparation mass fraction is the ammonia spirit of 8%-27%；
Step (2); titanium tetrachloride is instilled in the ammonia spirit of preparation with the constant pressure funnel that external exsiccator is protected; dripping the silver nitrate solution that molar concentration is 0.03-0.6mol/L that mole is titanium tetrachloride mole 0.017-0.3 times after dripping, continuously stirred 15-40min obtains solution A；
Step (3), adds solution A in reactor, adds the dodecyl sodium sulfate that quality is solution A quality 0.2%-1.5%, sonic oscillation 12-17min, is subsequently placed in the drying baker of 30-120 DEG C reaction 3-26h；
Step (4), room temperature is naturally cooled to after reaction completely, take out centrifugation precipitate, washing and ethanol purge successively, it is placed in again in vacuum drying oven and obtains presoma in 40-85 DEG C of dry 2-10h, then presoma is placed in ball milling 20-60min in ball mill mixes silver presoma to the nano titanium oxide forming 200-500 mesh；
Step (5), nano titanium oxide is mixed silver presoma and is placed in Muffle furnace calcining, use temperature programming, it is warming up to 160-250 DEG C of calcining 1-8h, it is warming up to 260-350 DEG C of calcining 1-8h, is warming up to 360-450 DEG C of calcining 1-8h, be warming up to 460-650 DEG C of calcining 3-8h, successively with water and ethanol purge after cooling, place into and drying baker obtains nano titanium oxide in 100-140 DEG C of dry 2-8h mix silver powder；
Step (6), nano titanium oxide is mixed silver powder joining mass ratio is in the deionized water that 200-1100 times of nano titanium oxide mixes silver powder quality, obtains nano titanium oxide in 20-70 DEG C of stirring 25min and mixes silver suspension；
Step (7), nano titanium oxide is mixed in the stearic acid ethanol solution that mass fraction is 11% that silver suspension adds and its mass ratio is 1.5-3:1,20-60min is stirred in 35-70 DEG C of constant temperature, reduce pressure sucking filtration again by above-mentioned mixed solution, and clean 2-4 time with deionized water, then in 30-80 DEG C of dry 1-4h, grind 20-50min after being cooled to room temperature and obtain stearic acid modified nano titanium oxide and mix aluminium powder；
Step (8), adding mass ratio in the abamectin emulsifiable concentrate that mass fraction is 5% is that the stearic acid modified nano titanium oxide of 0.017-0.05 times of abamectin emulsifiable concentrate mixes aluminium powder and mass ratio is the Ketohexamethylene of 0.01-0.4 times of abamectin emulsifiable concentrate, add and the deionized water solution containing the sodium lauryl sulphate that mass fraction is 10% that above-mentioned solution total mass ratio is 1-3:1, then obtain nano titanium oxide in 20-60 DEG C of stirring mixing 40-80min and mix the compound avilamycin pesticide of silver.
Nano titanium oxide of the present invention mixes the compound avilamycin pesticide of silver, prepares according to the method described above.
The process of the present invention is simple, it is easy to industrialized production, and obtained nano titanium oxide is mixed the compound avilamycin pesticide of silver and had environmental friendliness and the advantage such as the chemical residual time is short.
Detailed description of the invention
Being described in further details the foregoing of the present invention by the following examples, but this should not being interpreted as, the scope of the above-mentioned theme of the present invention is only limitted to below example, all technology realized based on foregoing of the present invention belong to the scope of the present invention.
Embodiment 1
1, preparation mass fraction is the ammonia spirit of 8%；
2, titanium tetrachloride is instilled in the ammonia spirit of preparation with the constant pressure funnel that external exsiccator is protected; dripping the silver nitrate solution that molar concentration is 0.03mol/L that mole is titanium tetrachloride mole 0.017 times after dripping, continuously stirred 15min obtains solution A；
3, solution A is added in reactor, add the dodecyl sodium sulfate that quality is solution A quality 0.2%, sonic oscillation 12min, be subsequently placed in the drying baker of 30 DEG C reaction 3h；
4, room temperature is naturally cooled to after reaction completely, take out centrifugation precipitate, washing and ethanol purge successively, then be placed in vacuum drying oven and obtain presoma in 40 DEG C of dry 2h, then presoma is placed in ball milling 20min in ball mill mixes silver presoma to forming nano titanium oxide；
5, nano titanium oxide is mixed silver presoma and is placed in Muffle furnace calcining, use temperature programming, it is warming up to 160 DEG C of calcining 1h, it is warming up to 260 DEG C of calcining 1h, it is warming up to 360 DEG C of calcining 1h, it is warming up to 460 DEG C of calcining 3h, successively with water and ethanol purge after cooling, places into and drying baker obtains nano titanium oxide in 100 DEG C of dry 2h mix silver powder；
6, nano titanium oxide is mixed silver powder joining mass ratio is in the deionized water that 200 times of nano titanium oxides mix silver powder quality, obtains nano titanium oxide in 20 DEG C of stirring 25min and mixes silver suspension；
7, nano titanium oxide is mixed in the stearic acid ethanol solution that mass fraction is 11% that silver suspension adds and its mass ratio is 1.5:1,20min is stirred in 35 DEG C of constant temperature, reduce pressure sucking filtration again by above-mentioned mixed solution, and clean 2 times with deionized water, then in 30 DEG C of dry 1h, grind 20min after being cooled to room temperature and obtain stearic acid modified nano titanium oxide and mix aluminium powder；
8, adding mass ratio in the abamectin emulsifiable concentrate that mass fraction is 5% is that the stearic acid modified nano titanium oxide of 0.017 times of abamectin emulsifiable concentrate mixes aluminium powder and Ketohexamethylene that mass ratio is 0.01 times of abamectin emulsifiable concentrate, add and the deionized water solution containing the sodium lauryl sulphate that mass fraction is 10% that above-mentioned solution total mass ratio is 1:1, then obtain nano titanium oxide in 20 DEG C of stirring mixing 40min and mix the compound avilamycin pesticide of silver.
Embodiment 2
1, preparation mass fraction is the ammonia spirit of 15%；
2, being instilled with the constant pressure funnel that external exsiccator is protected by titanium tetrachloride in the ammonia spirit of preparation, drip the silver nitrate solution that molar concentration is 0.3mol/L that mole is titanium tetrachloride mole 0.15 times after dripping, continuously stirred 25min obtains solution A；
3, solution A is added in reactor, add the dodecyl sodium sulfate that quality is solution A quality 0.8%, sonic oscillation 15min, be subsequently placed in the drying baker of 90 DEG C reaction 18h；
4, room temperature is naturally cooled to after reaction completely, take out centrifugation precipitate, washing and ethanol purge successively, then be placed in vacuum drying oven and obtain presoma in 60 DEG C of dry 6h, then presoma is placed in ball milling 40min in ball mill mixes silver presoma to forming nano titanium oxide；
5, nano titanium oxide is mixed silver presoma and is placed in Muffle furnace calcining, use temperature programming, it is warming up to 200 DEG C of calcining 4h, it is warming up to 300 DEG C of calcining 4h, it is warming up to 400 DEG C of calcining 4h, it is warming up to 550 DEG C of calcining 5h, successively with water and ethanol purge after cooling, places into and drying baker obtains nano titanium oxide in 120 DEG C of dry 6h mix silver powder；
6, nano titanium oxide is mixed silver powder joining mass ratio is in the deionized water that 600 times of nano titanium oxides mix silver powder quality, obtains nano titanium oxide in 50 DEG C of stirring 25min and mixes silver suspension；
7, nano titanium oxide is mixed in the stearic acid ethanol solution that mass fraction is 11% that silver suspension adds and its mass ratio is 2:1,40min is stirred in 50 DEG C of constant temperature, reduce pressure sucking filtration again by above-mentioned mixed solution, and clean 3 times with deionized water, then in 50 DEG C of dry 3h, grind 30min after being cooled to room temperature and obtain stearic acid modified nano titanium oxide and mix aluminium powder；
8, adding mass ratio in the abamectin emulsifiable concentrate that mass fraction is 5% is that the stearic acid modified nano titanium oxide of 0.035 times of abamectin emulsifiable concentrate mixes aluminium powder and Ketohexamethylene that mass ratio is 0.2 times of abamectin emulsifiable concentrate, add and the deionized water solution containing the sodium lauryl sulphate that mass fraction is 10% that above-mentioned solution total mass ratio is 2:1, then obtain nano titanium oxide in 40 DEG C of stirring mixing 60min and mix the compound avilamycin pesticide of silver.
Embodiment 3
1, preparation mass fraction is the ammonia spirit of 27%；
2, being instilled with the constant pressure funnel that external exsiccator is protected by titanium tetrachloride in the ammonia spirit of preparation, drip the silver nitrate solution that molar concentration is 0.6mol/L that mole is titanium tetrachloride mole 0.3 times after dripping, continuously stirred 40min obtains solution A；
3, solution A is added in reactor, add the dodecyl sodium sulfate that quality is solution A quality 1.5%, sonic oscillation 17min, be subsequently placed in the drying baker of 120 DEG C reaction 26h；
4, room temperature is naturally cooled to after reaction completely, take out centrifugation precipitate, washing and ethanol purge successively, then be placed in vacuum drying oven and obtain presoma in 85 DEG C of dry 10h, then presoma is placed in ball milling 60min in ball mill mixes silver presoma to forming nano titanium oxide；
5, nano titanium oxide is mixed silver presoma and is placed in Muffle furnace calcining, use temperature programming, it is warming up to 250 DEG C of calcining 8h, it is warming up to 350 DEG C of calcining 8h, it is warming up to 450 DEG C of calcining 8h, it is warming up to 650 DEG C of calcining 8h, successively with water and ethanol purge after cooling, places into and drying baker obtains nano titanium oxide in 140 DEG C of dry 8h mix silver powder；
6, nano titanium oxide is mixed silver powder joining mass ratio is in the deionized water that 1100 times of nano titanium oxides mix silver powder quality, obtains nano titanium oxide in 70 DEG C of stirring 25min and mixes silver suspension；
7, nano titanium oxide is mixed in the stearic acid ethanol solution that mass fraction is 11% that silver suspension adds and its mass ratio is 3:1,60min is stirred in 70 DEG C of constant temperature, reduce pressure sucking filtration again by above-mentioned mixed solution, and clean 4 times with deionized water, then in 80 DEG C of dry 4h, grind 50min after being cooled to room temperature and obtain stearic acid modified nano titanium oxide and mix aluminium powder；
8, adding mass ratio in the abamectin emulsifiable concentrate that mass fraction is 5% is that the stearic acid modified nano titanium oxide of 0.05 times of abamectin emulsifiable concentrate mixes aluminium powder and Ketohexamethylene that mass ratio is 0.4 times of abamectin emulsifiable concentrate, add and the deionized water solution containing the sodium lauryl sulphate that mass fraction is 10% that above-mentioned solution total mass ratio is 3:1, then obtain nano titanium oxide in 60 DEG C of stirring mixing 80min and mix the compound avilamycin pesticide of silver.
Comparative example 1
Step 1-3 is same as in Example 2, and in step 4 in addition to removing and adding the step that stearic acid modified nano titanium oxide mixes aluminium powder, other is consistent with the step 4 in embodiment 2.
The absorbance of the different pesticide of table 1 and the rate of settling
| Absorbance | The rate of settling (stability) | |
| Embodiment 1 | Within 0.378(50 minute, do not stop to stir lower illumination) | Within 36 minutes, do not settle or be layered |
| Embodiment 2 | Within 0.376(50 minute, do not stop to stir lower illumination) | Within 48 minutes, do not settle or be layered |
| Embodiment 3 | Within 0.374(50 minute, do not stop to stir lower illumination) | Within 34 minutes, do not settle or be layered |
| Comparative example 1 | Within 0.545(50 minute, do not stop to stir lower illumination) | Sedimentation layering in 3 minutes |
Find that comparative example does not have good stability by table 1, within 3 minutes, i.e. start significantly to settle layering, find that the dulling luminosity ratio embodiment of comparative example is the most many by the contrast of absorbance, illustrate to be not added with nano titanium oxide to mix its photocatalytic degradation of silver and change hardly very slowly, and embodiment 1-3 is relatively good.Illustrate that the product prepared according to the present invention all shows excellence in terms of stability, photocatalytic degradation.
Embodiment above describes the ultimate principle of the present invention, principal character and advantage; skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; the principle that the present invention is simply described described in above-described embodiment and description; under the scope without departing from the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements each fall within the scope of protection of the invention.
Claims (2)
1. a nano titanium oxide mixes the silver-colored preparation method being combined avilamycin pesticide, it is characterised in that concretely comprise the following steps:
Step (1), preparation mass fraction is the ammonia spirit of 8%-27%；
Step (2); titanium tetrachloride is instilled in the ammonia spirit of preparation with the constant pressure funnel that external exsiccator is protected; dripping the silver nitrate solution that molar concentration is 0.03-0.6mol/L that mole is titanium tetrachloride mole 0.017-0.3 times after dripping, continuously stirred 15-40min obtains solution A；
Step (3), adds solution A in reactor, adds the dodecyl sodium sulfate that quality is solution A quality 0.2%-1.5%, sonic oscillation 12-17min, is subsequently placed in the drying baker of 30-120 DEG C reaction 3-26h；
Step (4), room temperature is naturally cooled to after reaction completely, take out centrifugation precipitate, washing and ethanol purge successively, it is placed in again in vacuum drying oven and obtains presoma in 40-85 DEG C of dry 2-10h, then presoma is placed in ball milling 20-60min in ball mill mixes silver presoma to the nano titanium oxide forming 200-500 mesh；
Step (5), nano titanium oxide is mixed silver presoma and is placed in Muffle furnace calcining, use temperature programming, it is warming up to 160-250 DEG C of calcining 1-8h, it is warming up to 260-350 DEG C of calcining 1-8h, is warming up to 360-450 DEG C of calcining 1-8h, be warming up to 460-650 DEG C of calcining 3-8h, successively with water and ethanol purge after cooling, place into and drying baker obtains nano titanium oxide in 100-140 DEG C of dry 2-8h mix silver powder；
Step (6), nano titanium oxide is mixed silver powder joining mass ratio is in the deionized water that 200-1100 times of nano titanium oxide mixes silver powder quality, obtains nano titanium oxide in 20-70 DEG C of stirring 25min and mixes silver suspension；
Step (7), nano titanium oxide is mixed in the stearic acid ethanol solution that mass fraction is 11% that silver suspension adds and its mass ratio is 1.5-3:1,20-60min is stirred in 35-70 DEG C of constant temperature, reduce pressure sucking filtration again by above-mentioned mixed solution, and clean 2-4 time with deionized water, then in 30-80 DEG C of dry 1-4h, grind 20-50min after being cooled to room temperature and obtain stearic acid modified nano titanium oxide and mix aluminium powder；
Step (8), adding mass ratio in the abamectin emulsifiable concentrate that mass fraction is 5% is that the stearic acid modified nano titanium oxide of 0.017-0.05 times of abamectin emulsifiable concentrate mixes aluminium powder and mass ratio is the Ketohexamethylene of 0.01-0.4 times of abamectin emulsifiable concentrate, add and the deionized water solution containing the sodium lauryl sulphate that mass fraction is 10% that above-mentioned solution total mass ratio is 1-3:1, then obtain nano titanium oxide in 20-60 DEG C of stirring mixing 40-80min and mix the compound avilamycin pesticide of silver.
2. a nano titanium oxide mixes the compound avilamycin pesticide of silver, it is characterised in that be to be prepared by the method described in claim 1.
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| CN110204823A (en) * | 2019-06-12 | 2019-09-06 | 金华市捷特包装有限公司 | A kind of high-performance rotational moulding case |
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Application publication date: 20160803 |